Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | HCID 57489636 | HCID 57489636 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 57489634 | HCID 57489634 | — |
Reaction Steps
A mixture of 6-chloro-2-(4-(methylsulfonyl)phenylamino)nicotinamide (19.4 mg, 0.060 mmol) and piperidine (2 mL) in a sealed tube was stirred in a 90° C. oil bath for 5 h. The mixture was diluted with EtOAc (25 mL), washed with saturated NH4Cl(2×5 mL), brine (5 mL), dried (MgSO4), and concentrated. After addition of CH2Cl2 (2 mL), white solid precipitated from the solution upon sitting. The solid was collected by filtration (14.1 mg, 60%). LCMS: (M+H)+=375.1. 1H NMR (400 MHz, acetone-d6) δ ppm 12.20 (1H, s), 7.90-8.09 (3H, m), 7.78-7.89 (2H, m), 6.33 (1H, d, J=8.78 Hz), 3.58-3.89 (4H, m), 3.07 (3H, s), 1.52-1.85 (6H, m).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08586751B2 |
|---|
| Source dataset | uspto-grants-2013_11 |
|---|
| ORD ID | ord-1e156e517cba4c3c808eb0a17c4fca1c |
|---|
| Source note | uspto-grants-2013_11 |
|---|